The Organic Chem Lab Survival Manual: A Student?s Guide to Techniques

Written for the laboratory that accompanies the sophomore/junior level courses in Organic Chemistry, Zubrick provides students with a valuable guide to the basic techniques of the Organic Chemistry lab. The book will help students understand and practice good lab safety. It will also help students become familiar with basic instrumentation, techniques and apparatus and help them master the latest techniques such as interpretation of infrared spectroscopy. The guide is mostly macroscale in its orientation. INDICE: CHAPTER 1 SAFETY FIRST, LAST, AND ALWAYS .Accidents Will Not Happen .Disposing of Waste .Material Safety Data Sheet (MSDS) .Green Chemistry and Planning an Organic Synthesis .An iBag for Your iThing .Exercises .CHAPTER 2 KEEPING A NOTEBOOK .A Technique Experiment .A Synthesis Experiment .The Six Maybe Seven Elements in Your Experimental Write–Up .The Acid Test .Notebook Mortal Sin .Calculation of Percent Yield (Not Yeild!) .Estimation Is Your Friend .Exercises .CHAPTER 3 INTERPRETING A HANDBOOK .Google and the WIKI .The Terphenyl Anomaly .Exercises .CHAPTER 4 JOINTWARE .Stoppers with Only One Number .Another Episode of Love of Laboratory .Hall of Blunders and Things Not Quite Right .The O–Ring and Cap Branch Out .Greasing the Joints .Storing Stuff and Sticking Stoppers .Corking a Vessel .CHAPTER 5 MICROSCALE JOINTWARE .Microscale: A Few Words .Uh–Oh Rings .The O–Ring Cap Seal .The Comical Vial (That s Conical!) .The Conical Vial as Vial .Packaging Oops .Tare to the Analytical Balance .The Electronic Analytical Balance .Heating These Vials .The Microscale Drying Tube .Gas Collection Apparatus .CHAPTER 6 OTHER INTERESTING EQUIPMENT .Funnels, and Beakers, and Flasks Oh My! .The Flexible Double–Ended Stainless Steel Spatula .CHAPTER 7 PIPET TIPS .Pre–Preparing Pasteur Pipets .Pipet Cutting .Pipet Filtering Liquids .Pipet Filtering Solids .CHAPTER 8 SYRINGES, NEEDLES, AND SEPTA .The Rubber Septum .CHAPTER 9 CLEAN AND DRY .Drying Your Glassware When You Don t Need To .Drying Your Glassware When You Do Need To .CHAPTER 10 DRYING AGENTS .Typical Drying Agents .Using a Drying Agent .Following Directions and Losing Product Anyway .Drying Agents: Microscale .Drying in Stages: The Capacity and Efficiency of Drying Agents .Exercises .CHAPTER 11 ON PRODUCTS .Solid Product Problems .Liquid Product Problems .The Sample Vial .Hold It! Don t Touch That Vial .CHAPTER 12 THE MELTING–POINT EXPERIMENT .Sample Preparation .M elting–Point Hints .The Mel–Temp Apparatus .The Fisher–Johns Apparatus .The Thomas–Hoover Apparatus .Operation of the Thomas–Hoover Apparatus .Using the Thiele Tube .Exercises .CHAPTER 13 RECRYSTALLIZATION .Finding a Good Solvent .General Guidelines for a Recrystallization .Gravity Filtration .The Buchner Funnel and Filter Flask .The Hirsch Funnel and Friends .Activated Charcoal .The Water Aspirator: A Vacuum Source .The Water Trap .Working with a Mixed–Solvent System The Good Part .A Mixed–Solvent System The Bad Part .Salting Out .World–Famous Fan–Folded Fluted Paper .Exercises .CHAPTER 14 RECRYSTALLIZATION: MICROSCALE .Isolating the Crystals .Craig Tube Filtration .Centrifuging the Craig Tube .Getting the Crystals Out .CHAPTER 15 EXTRACTION AND WASHING .Never–Ever Land .Starting an Extraction .Dutch Uncle Advice .The Separatory Funnel .The Stopper .The Teflon Stopcock .How to Extract and Wash What .The Road to Recovery Back–Extraction .A Sample Extraction .Performing an Extraction or Washing .Extraction Hints .Exercises .CHAPTER 16 EXTRACTION AND WASHING: MICROSCALE .Mixing .Separation: Removing the Bottom Layer .Separation: Removing the Top Layer .Separation: Removing Both Layers .CHAPTER 17 SOURCES OF HEAT .Boiling Stones .The Steam Bath .The Bunsen Burner .The Heating Mantle .Proportional Heaters and Stepless Controllers .Exercise .CHAPTER 18 CLAMPS AND CLAMPING .Clamping a Distillation Setup .Clipping a Distillation Setup .CHAPTER 19 DISTILLATION .Distillation Notes .Class 1: Simple Distillation .The Distillation Example .The Distillation Mistake .Class 2: Vacuum Distillation .Class 3: Fractional Distillation .Azeotropes .Class 4: Steam Distillation .Steam Distillation Notes .Simulated Bulb–to–Bulb Distillation: Fakelrohr .Exercises .CHAPTER 20 MICROSCALE DISTILLATION .Like the Big Guy .Microscale Distillation II: The Hickman Still .The Hickman Still Setup .Hickman Still Heating .Recovering Your Product .A Port in a Storm .CHAPTER 21 THE ROTARY EVAPORATOR .Exercises .CHAPTER 22 REFLUX AND ADDITION .Standard Reflux .A Dry Reflux .Addition and Reflux .Exercise .CHAPTER 23 REFLUX: MICROSCALE .Addition and Reflux: Microscale .CHAPTER 24 SUBLIMATION .CHAPTER 25 MICROSCALE BOILING POINT .Microscale Boiling Point .Ultramicroscale Boiling Point .CHAPTER 26 CHROMATOGRAPHY: SOME GENERALITIES .Adsorbents .Separation or Development .The Eluatropic Series .CHAPTER 27 THIN–LAYER CHROMATOGRAPHY: TLC .We Don t Make Our Own TLC Plates Any More, But... .The Plate Spotter .Spotting the Plates .Developing a Plate .Visualization .Interpretation .Multiple Spotting .Cospotting .Other TLC Problems .Preparative TLC .Exercises .CHAPTER 28 WET–COLUMN CHROMATOGRAPHY .Preparing the Column .Compounds on the Column .Visualization and Collection .Wet–Column Chromatography: Microscale .Flash Chromatography .Microscale Flash Chromatography .Exercises .CHAPTER 29 REFRACTOMETRY .The Abbé Refractometer .Before Using the Abbé Refractometer: A Little Practice .Using the Abbé Refractometer .Refractometry Hints .CHAPTER 30 GAS CHROMATOGRAPHY .The Mobile Phase: Gas .GC Sample Preparation .GC Sample Introduction .Sample in the Column .Sample at the Detector .Electronic Interlude .Sample on the Computer .Parameters, Parameters .Exercises .CHAPTER 31 HP LIQUID CHROMATOGRAPHY .The Mobile Phase: Liquid .HPLC Sample Preparation .HPLC Sample Introduction .Sample in the Column .Sample at the Detector .Sample on the Computer .Parameters, Parameters .Exercises .CHAPTER 32 INFRARED SPECTROSCOPY (AND A BIT OF UV–VIS, TOO) .Molecules as Balls on Springs .Ah, Quantum Mechanics .The Dissonant Oscillator .But Wait! There s More .More Complicated Molecules .Correlation Tables to the Rescue .Troughs and Reciprocal Centimeters .Some Functional Group Analysis .A Systematic Interpretation .Infrared Sample Preparation .Running the Spectrum .The Fourier Transform Infrared (FTIR) .A Reflectance Attachment: Something to Think About .And UV–VIS Too! .Electrons Get to Jump .Instrument Configuration .Exercises .CHAPTER 33 NUCLEAR MAGNETIC RESONANCE .Nuclei Have Spin, Too .The Magnetic Catch .Everybody Line Up, Flip, and Relax .A More Sensitive Census .The Chemical Shift .T for One and Two .Be It Better Resolved . . . .Incredibly Basic FT–NMR .NMR Sample Preparation .Some NMR Terms and Interpretations .CHAPTER 34 THEORY OF DISTILLATION .Class 1: Simple Distillation .Class 3: Fractional Distillation .Class 4: Steam Distillation .INDEX

• ISBN: 978-1-118-87578-0
• Editorial: John Wiley & Sons
• Encuadernacion: Rústica
• Páginas: 314
• Fecha Publicación: 25/11/2015
• Nº Volúmenes: 1
• Idioma: Inglés